Search

The objective of the present work was to develop a sensitive, selective, accurate and precise stability-indicating HPLC method for quantification of degradation products and process-related impurities in fesoterodine fumarate extended-release tablets. The degradation profile was studied by conducting forced degradation studies and all the degradation products formed during degradation were separated. A chromatographic separation was achieved by using Waters Symmetry C18, 250 × 4.6 mm, 5 μm column, maintained at 30°C. Mobile phase A (0.05% trifluoroacetic acid in water) and mobile phase B (90% of 0.02% TFA in methanol and 10% of water) were used in gradient elution mode. A total of 75 μL of each solution was injected and peak responses were quantified at 220 nm. The method was found specific, precise, accurate, linear, rugged, robust and sensitive. During stability studies of fesoterodine fumarate extended-release tablets, one unknown impurity at relative retention time 1.37 was found increasing beyond the identification threshold. This impurity was isolated by using Preparative HPLC and structure was elucidated using mass and NMR spectroscopy. This method is a simple, inexpensive HPLC method that can be used as a routine quality control test for the estimation of impurities in fesoterodine fumarate extended-release tablets. [ABSTRACT FROM AUTHOR]

The objective of the current research is to understand the degradation behavior of avanafil under different stress conditions and to develop a stability-indicating high-performance liquid chromatography (HPLC) method for simultaneous determination of degradants observed during degradation. Avanafil tablets were exposed to acid, base, water, oxidative, thermal, and photolytic degradation conditions. In acid, oxidative, thermal, and humidity degradation, significant degradation was observed. All the degradants observed during degradation were separated from known impurities of avanafil by using reverse-phase (RP)-HPLC. Mobile phase A, 0.1% trifluoro acetic acid and triethylamine in water, and mobile phase B, water and acetonitrile in the ratio of 20:80 (v/v), were used at a flow rate of 1.2 mL/min in gradient elution mode. Separation was achieved by using Inertsil ODS 3 column (3 μm, 4.6 mm × 250 mm) at 45 °C. Peak responses were recorded at 245 nm. Method capability for detecting and quantifying the degradants, which can form during stability, was proved by demonstrating the peak purity of avanafil peak in all the stressed samples. Mass balance was established by performing the assay of stressed sample against reference standard. Mass balance was found >97% for all the stress conditions. The developed analytical method was validated as per International Conference on Harmonization (ICH) guidelines. The method was found specific, linear, accurate, precise, rugged, and robust. [ABSTRACT FROM AUTHOR]